LEADER 05227oam 2200625Ia 450 001 9910782367303321 005 20231102200804.0 010 $a1-281-76266-0 010 $a9786611762667 010 $a0-08-095152-X 010 $a0-08-055819-4 035 $a(CKB)1000000000547726 035 $a(EBL)404862 035 $a(OCoLC)476220392 035 $a(SSID)ssj0000211489 035 $a(PQKBManifestationID)12043443 035 $a(PQKBTitleCode)TC0000211489 035 $a(PQKBWorkID)10311844 035 $a(PQKB)11631291 035 $a(MiAaPQ)EBC404862 035 $a(PPN)182574830 035 $a(EXLCZ)991000000000547726 100 $a20080630d2008 uy 0 101 0 $aeng 135 $aur|n|---||||| 181 $ctxt$2rdacontent 182 $cc$2rdamedia 183 $acr$2rdacarrier 200 00$aNMR spectroscopy in pharmaceutical analysis /$fedited by Ulrike Holzgrabe, Iwona Wawer, Bernd Diehl 210 1$aBurlington :$cElsevier,$d2008. 215 $a1 online resource (525 pages) 311 0 $a0-444-53173-4 320 $aIncludes bibliographical references and index. 327 $aFront Cover; NMR Spectroscopy in Pharmaceutical Analysis; Copyright Page; Table of Contents; Preface; List of Contributors; List of Editors; Part I FUNDAMENTALS AND TECHNIQUES; Chapter 1 Principles in NMR Spectroscopy; 1 Short History; 2 The NMR Experiment; 2.1 Excitation, relaxation and sensitivity; 2.2 Relaxation; 3 Chemical Shift; 3.1 Electronic density; 3.2 Anisotropy; 3.3 Mesomerism; 3.4 Steric effects; 4 Calibration and Relative Scale ppm; 5 Spin-Spin Coupling; 5.1 The coupling constant; 5.2 Multiplicity; 5.3 Roof effect; 5.4 Angular dependence of the coupling constant 327 $a5.5 Heteronuclear coupling; 5.6 13C NMR satellites in 1H NMR spectra; 6 Heteronuclear Spectra; 6.1 Decoupling; 6.2 Quantitative heteronuclear NMR; 7 Molecular Dynamics; 7.1 Deuterium exchange and solvent effects; 8 Chemical Derivatisation; 9 Stereochemistry; 9.1 Diastereomerism; 9.2 Atrop or axial chirality; 9.3 Enantiomeric excess; 9.4 Diastereotopy; 10 Two-dimensional Methods for Structure Elucidation; 11 Experimental Data; Chapter 2 Quantitative NMR in the Solution State NMR; 1 Introduction; 2 Basics; 3 Quantitative NMR Spectroscopy; 3.1 Relative method; 3.2 Absolute method; 4 Validation 327 $a4.1 Linearity; 4.2 Robustness; 4.3 Specificity and selectivity; 4.4 Accuracy; 4.5 Precision; 4.6 Measurement uncertainty; 4.7 Round robin tests; 5 Sensitivity; 6 Conclusion; Chapter 3 qNMR in Solid State; 1 Introduction to Solid-state NMR; 2 Quantitative Aspects of Solid-state NMR, Protocol for Quantitation; 3 An Example: Quantitation of Pseudoephedrine in Dosage Form; 4 Quantitation of Polymorphs and Formulated Drugs; Chapter 4 Microcoil Nuclear Magnetic Resonance Spectroscopy; 1 Introduction; 2 Intrinsic NMR Sensitivity; 3 Development of Small Coils for High-Resolution NMR 327 $a3.1 Saddle/Helmholtz coils; 3.2 Solenoidal coils; 3.3 Planar RF coils; 3.4 Novel microcoil designs; 3.5 High-temperature superconducting microprobes; 4 Sensitivity Comparisons; 5 Nanoliter Volume Applications of RF Microcoils - Hyphenated cITP-NMR; 6 Microliter Volume Applications of RF Microcoils; 6.1 Helmholtz/saddle coils; 6.2 Solenoidal coils; 6.3 Superconducting microcoils; 7 Hyphenation of Microseparation Techniques with Microliter NMR Detection; 8 Multiple Coil Probeheads; 9 Solid-State Applications of Small Coils; 10 Conclusion 327 $aChapter 5 qNMR Spectroscopy in Drug Analysis - A General View; 1 Introduction; 2 NMR Spectroscopy in International Pharmacopoeias; 2.1 Identification of drugs; 2.2 Tests; 2.3 Assay; 3 Validation; 4 Conclusions; Part II GENERAL APPLICATIONS; Chapter 1 Investigation of Multi-Component Drugs by NMR Spectroscopy; 1 Introduction; 1.1 Solvent; 1.2 pH value; 1.3 Temperature; 1.4 Auxiliary reagents; 1.5 Limitations; 2 Codergocrine Mesylate; 2.1 1H NMR spectroscopy; 2.2 13C NMR spectroscopy; 2.3 High-performance liquid chromatography; 2.4 HPLC versus NMR spectroscopy; Chapter 2 NMR Applications for Polymer Characterisation 330 $aFor almost a decade, quantitative NMR spectroscopy (qNMR) has been established as valuable tool in drug analysis. In all disciplines, i. e. drug identification, impurity profiling and assay, qNMR can be utilized. Separation techniques such as high performance liquid chromatography, gas chromatography, super fluid chromatography and capillary electrophoresis techniques, govern the purity evaluation of drugs. However, these techniques are not always able to solve the analytical problems often resulting in insufficient methods. 606 $aNuclear magnetic resonance spectroscopy 606 $aDrugs$xAnalysis 615 0$aNuclear magnetic resonance spectroscopy. 615 0$aDrugs$xAnalysis. 676 $a615.19 676 $a615.1901 701 $aHolzgrabe$b U$g(Ulrike)$0935735 701 $aWawer$b I$g(Iwona)$0312861 701 $aDiehl$b B$g(Bernd)$0935736 801 0$bMiAaPQ 801 1$bMiAaPQ 801 2$bMiAaPQ 906 $aBOOK 912 $a9910782367303321 996 $aNMR spectroscopy in pharmaceutical analysis$93768189 997 $aUNINA